CN105130078B - Compound sedimentation agent, twin crystal centrifuge body and technique for the treatment of the sodium sulfonate technique waste water of DMIP 5 - Google Patents
Compound sedimentation agent, twin crystal centrifuge body and technique for the treatment of the sodium sulfonate technique waste water of DMIP 5 Download PDFInfo
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- CN105130078B CN105130078B CN201510562570.4A CN201510562570A CN105130078B CN 105130078 B CN105130078 B CN 105130078B CN 201510562570 A CN201510562570 A CN 201510562570A CN 105130078 B CN105130078 B CN 105130078B
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- waste water
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- dimethyl isophthalate
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Abstract
The invention discloses a kind of compound sedimentation agent, twin crystal centrifuge body and technique processed for the sodium sulfonate technique waste water of DMIP 5；Sedimentation agent is wherein combined to be made up of ethylene glycol and glycerine mixing, it will not react in the neutral, solution of low temperature with the material of other in solution, and the solubility of three monomers and sodium sulphate in water can be effectively reduced so that three monomers and sulfate crystal in concentrate are separated out；Separation of solid and liquid is carried out by being provided with the twin crystal centrifuge body of Double layer rotating filter assemblies simultaneously, it can be ingenious, simple and practical by feed separation after sedimentation into sodium sulphate, thick three monomer and the sedimentation agent aqueous solution, separate mode design, enormously simplify separating technology；And whole processing procedure of the invention is physical process, without chemical process, will not produce new material, will not also produce new waste water, can substantially realize that three monomers produce wastewater zero discharge, and considerable benefit, with high economic benefit and environmental benefit.
Description
Technical field
The present invention relates to chemical wastewater treatment technical field, and in particular to a kind of rutgers -5- sodium sulfonates
The processing equipment and technique of technique waste water.
Background technology
Sodium Dimethyl Isophthalate-5-sulfonate（It is commonly called as three monomers）, molecular formula is C10H9O2SNa, is mainly used in synthesis
Cation dyeable polyester（CDP）Third monomer, make CDP polyester fibers that there is good affine performance to cation fuel, make
CDP fibers can be with dyeing at normal pressure, and bright color after being dyed, chromatogram are complete, color fastness is high, not fugitive color, and with good
Antistatic behaviour, hygroscopicity, anti-pilling and gas permeability, it is comfortable and easy to wear.Production method be using various concentrations oleum or
Sulfur trioxide carries out sulfonation to M-phthalic acid, then is neutralized through methanol esterification, soda ash or caustic soda, separated, refined and product is obtained；
The waste water that the generation of three monomers is washed after the mother liquor of separation process generation and separation is respectively provided with high salt, the wherein characteristic of COD high, sulphur
The content of sour sodium is 5% or so, and the content of three monomers is 4% or so, and round being substantially salt, but currently available technology does not have also
Clear and definite technological means can be separated the two by after crystallization；Therefore, the processing method of current three monomer process waste water
All in experimental stage, prior art is more based on extraction, this method high cost, but also produces new waste water, it is impossible to by three
Monomer manufacturing enterprise is received.But three monomer process waste water are expelled directly out system, and environment is polluted；Therefore it is how right
Three monomer process waste water recycled the always puzzlement industry realize energy-saving and emission-reduction, one of clean manufacturing great ask
Topic.
The content of the invention
It is an object of the invention to provide a kind of for the compound of Sodium Dimethyl Isophthalate-5-sulfonate technique waste water treatment
Sedimentation agent, twin crystal centrifuge body and waste water Comprehensive recycle technology, solve three monomer process waste water in the prior art and are difficult to
The problem of recycling.
The present invention provides a kind of compound sedimentation for the treatment of Sodium Dimethyl Isophthalate-5-sulfonate technique waste water first
Agent, it is applied to one in three monomer process waste water can reduce solubility of the sodium sulphate in water and crystallize precipitation and can increase
The crystalline particle of big sodium sulphate, secondly can reduce solubility of three monomers in water and crystallize precipitation, finally realizes sodium sulphate
Precipitation is crystallized with three monomers and the two particle diameter occurs that obvious gradient, i.e. sulfate crystal particle be big, three monomer crystalline particles are small；
Above-mentioned compound sedimentation agent is specifically comprised：By ethylene glycol and glycerine according to mass ratio 5:5~7:3 mix；Further preferably
For：The mass ratio of the ethylene glycol and glycerine is 6:4.
Secondly the present invention provide it is a kind of for Sodium Dimethyl Isophthalate-5-sulfonate technique waste water treatment bicrystal from
Scheming, twin crystal centrifuge body be used for by sedimentation after the sodium sulphate for obtaining, low three monomer separated according to particle diameter difference, its skill
Art scheme is：Double layer rotating filter assemblies including being spaced suit in body and its successively, the Double layer rotating filter assemblies
Be co-axially mounted and be connected with motor by transmission mechanism, and wherein on internal layer rotating filter component filter medium aperture
More than the aperture of filter medium on outer layer rotating filter component.Preferably, the filter medium on the internal layer rotating filter component
For the filter medium on screen pack, outer layer rotating filter component is filter cloth；The outer layer rotating filter component is rotated through with internal layer
The rotating ratio for filtering component is 6:1.The principle of twin crystal centrifuge body is based on having taken into full account that sulfate crystal particle is big, three monomers
The small characteristic of crystalline particle, therefore two-layer filtration is devised, realize sulfuric acid by setting the different filter medium in aperture
Sodium and three monomers are individually separated, overcome existing conventional centrifuge can only realize single solid-liquid difference and can not be in solid-liquid
The drawbacks of while separation to the crystalline solid separated in synchronization of different-grain diameter.Certainly, the range of application of above-mentioned twin crystal centrifuge body is not
Be limited to the separation of sodium sulphate and three monomer crystalline solid in the present invention, it is also possible to suitable for other industry be similar to separation demand, together
When be that mentality of designing has been opened up in the separation of various crystallized stocks.
Then we provide a kind of Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology, its
Comprise the following steps that, and wherein step（2）The compound sedimentation agent that sedimentation operation is used is compound sedimentation agent mentioned above：
（1）, evaporization process：After by three monomer process waste water rectifying methanol removals, it is concentration to be evaporated and be concentrated into volume
The 30-40% of front volume, wherein evaporating the steam condensate (SC) for obtaining switchs to process water reuse, the concentrate that evaporation and concentration is obtained
It is transferred to next procedure；
（2）, sedimentation operation：The concentrate that evaporization process is obtained is cooled to 30-35 degree, is then added thereto to account for its body
The compound sedimentation agent of product 3-5%, then crystallizes under agitation；Separation circuit is sent under conditions of stirring afterwards；During the crystallization
Between be preferably 1 hour；
（3）, separation circuit：Isophthalic is obtained by being individually separated according to particle diameter difference by the concentrate after sedimentation operation treatment
Dicarboxylic acid dimethyl ester -5- sulfonic acid sodium crystal, sodium sulfate crystal and mother liquor；Then by Sodium Dimethyl Isophthalate-5-sulfonate
Crystal goes to refining step to carry out refinement treatment and obtains finished product, and isolated mother liquor is gone into compound sedimentation agent recovery process；
（4）, compound sedimentation agent recovery process：The mother liquor that separation circuit is obtained reclaims compound sedimentation by rectification process
Agent；Compound sedimentation agent after recovery goes to step（2）Recycle.
Obtained to further improve above-mentioned Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology
To the utilization rate of the recovery quality, yield and Treated sewage reusing of product, we are further improved to such scheme：
The step（3）In refinement treatment be to lead to isolated Sodium Dimethyl Isophthalate-5-sulfonate crystal
Cross water-washing method to be refined, the wash water in the washing comes from step（1）The steam condensate (SC) that evaporization process is obtained.Due to
The steam condensate (SC) that evaporation is obtained, its cleanliness factor is very high, is fully able to be directly used in three monomer washing process, both realizes technique
The reuse of water, reduce the consumption of fresh water, at the same also can guarantee that three monomers it is refined after product quality.
The step（3）Isolated sodium sulfate crystal is refined by water-washing method, washes the waste water set for producing
With to step（1）Three monomer process waste water in.Purity can reach 99% after the sodium sulfate crystal that above-mentioned washing is refined is dried
More than.
The step（1）The evaporation concentration equipment that middle evaporization process is used is Mvr evaporators；The step（1）Middle evaporation
It is the 35% of condensate precursor product to be evaporated three monomer process waste water in operation and be concentrated into volume.
The step（4）In be combined the bed material recovery after sedimentation agent recovery process rectification process to step（1）In
In three monomer process waste water.
Compound sedimentation agent in the present invention will not occur anti-in the neutral, solution of low temperature with the material of other in solution
Should, and the solubility of three monomers and sodium sulphate in water can be effectively reduced so that three monomers and sodium sulphate in concentrate
Crystallization is separated out；Simultaneously by twin crystal centrifuge body can by sedimentation after feed separation into sodium sulphate, thick three monomer and sedimentation agent
The aqueous solution, separate mode design is ingenious, simple and practical, enormously simplify separating technology；By comprehensive reutilization of the invention
After PROCESS FOR TREATMENT, the rate of recovery of three monomers and sodium sulphate respectively reaches more than 93% in three monomer process waste water（Highest is more than 95%）
With more than 90%（Highest is more than 93%）, it is refined after three monomers reach top grade standard, it is refined after sodium sulfate crystal purity can reach
More than 99%, and whole processing procedure is physical process, without chemical process, will not produce new material, will not also produce new
Waste water, can substantially realize that three monomers produce wastewater zero discharge, and considerable benefit, with high economic benefit and environment
Benefit.
Brief description of the drawings
Fig. 1 is the process chart of Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology；
Fig. 2 is the structural representation of twin crystal centrifuge body；
In figure：1st, body, 2, outer layer rotating filter component, 3, internal layer rotating filter component, 4, power transmission shaft, 5, drive electricity
Machine.
Specific embodiment
The present invention is further illustrated with reference to specific specific embodiment.Embodiment 1-3 steps（2）In it is double
Crystal centrifuge structure is as follows：Double layer rotating filter assemblies including being spaced suit in body and its successively, Double layer rotating mistake
Filter component is co-axially mounted and is connected with motor by transmission mechanism, outer layer rotating filter component and internal layer rotating filter group
The rotating ratio of part is 6:1；And the aperture of filter medium is more than on outer layer rotating filter component wherein on internal layer rotating filter component
The aperture of filter medium.Filter medium on internal layer rotating filter component is screen pack, the filtering on outer layer rotating filter component
Medium is filter cloth.
Embodiment 1
A kind of Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology, comprises the following steps：
（1）, evaporization process：After three monomer process waste water rectifying methanol removals（Wherein the content of sodium sulphate is 5%, and three is single
The content of body is 4%）, it is the 35% of condensate precursor product to be evaporated by MVR evaporators and be concentrated into volume, wherein what evaporation was obtained
Steam condensate (SC) switchs to process water reuse, and the concentrate that evaporation and concentration is obtained is transferred to next procedure；
（2）, sedimentation operation：The concentrate that evaporization process is obtained is cooled to 30-35 degree, is then added thereto to account for its body
The compound sedimentation agent of product 3-5%, then crystallizes 1 hour under agitation；Separation circuit is sent under conditions of stirring afterwards；It is described
Compound sedimentation agent is by ethylene glycol and glycerine according to mass ratio 6:4 mix；
（3）, separation circuit：Will be isolated by bicrystal centrifuge by the concentrate after sedimentation operation treatment
Sodium Dimethyl Isophthalate-5-sulfonate crystal, sodium sulfate crystal and mother liquor；By isolated M-phthalic acid diformazan
Ester -5- sulfonic acid sodium crystal carries out being refining to obtain finished product by water-washing method, and the wash water in washing comes from step（1）Evaporization process
The steam condensate (SC) for obtaining；Isolated sodium sulfate crystal is refined by water-washing method, the waste water set for producing is washed
With to step（1）Three monomer process waste water in；Isolated mother liquor is gone into compound sedimentation agent recovery process；
（4）, compound sedimentation agent recovery process：The mother liquor that separation circuit is obtained reclaims compound sedimentation by rectification process
Agent；Compound sedimentation agent after recovery goes to step（2）Recycle；Bed material recovery after rectification process is to step（1）In
Three monomer process waste water in.
Embodiment 2
A kind of Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology, its step and embodiment 1
It is basically identical, differ only in and be combined in the present embodiment sedimentation agent by ethylene glycol and glycerine according to mass ratio 5:5 mixing and
Into.
Embodiment 3
A kind of Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology, its step and embodiment 1
It is basically identical, differ only in and be combined in the present embodiment sedimentation agent by ethylene glycol and glycerine according to mass ratio 7:3 mixing and
Into.
Three monomers and the yield of sodium sulphate that are obtained to embodiment 1-3 individually below, purity carry out calculating analysis, as a result
See the table below.
| Three monomer yield % | Three monomer indexs | Sodium sulphate yield % | Sodium sulphate purity % | Ethylene glycol：Glycerine | |
| Embodiment 1 | 95.1 | Top grade | 93.2 | ≥99 | 6:4 |
| Embodiment 2 | 93 | Top grade | 90.5 | ≥99 | 7:3 |
| Embodiment 3 | 94.3 | Top grade | 92.1 | ≥99 | 5:5 |
It is attached：The technical indicator of three monomer top grade product
Colourity≤20
Absorbance≤0.05
Acid number（mgKOH/g）≤0.6
Saponification number（mgKOH/g）376-380
Sulfate radical（In terms of sodium sulphate, mg/kg）≤100
Iron content（In terms of Fe, mg/kg）≤4
Moisture（Mass fraction, %）≤0.4
Chlorion（mg/kg）≤15.
Above example is only part preferred scheme of the invention, visible by above table, is returned by synthesis of the invention
Receive using after PROCESS FOR TREATMENT, the rate of recovery of three monomers and sodium sulphate respectively reaches more than 93% in three monomer process waste water（It is most superb
Cross 95%）With more than 90%（Highest is more than 93%）, it is refined after three monomers reach top grade standard, sodium sulfate crystal purity after refining
More than 99% is can reach, the wherein technique effect of embodiment 1 is optimal, can be as optimal technical scheme.In protection of the invention
Within the scope of, above-mentioned each technical characteristic is reassembled into other technical schemes by others skilled in the art completely, with this programme
Realize solving same technical problem, realize identical purpose, be considered as identical with this claims substance, each fall within this right
Within the protection domain of claim.
Claims (7)
1. a kind of Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology, it is characterised in that including with
Lower step：
（1）, evaporization process：After by Sodium Dimethyl Isophthalate-5-sulfonate technique waste water rectifying methanol removal, it is evaporated dense
It is the 30-40% of condensate precursor product to be reduced to volume, wherein evaporating the steam condensate (SC) for obtaining switchs to Comprehensive recycle technology water
Reuse, the concentrate that evaporation and concentration is obtained is transferred to next procedure；
（2）, sedimentation operation：The concentrate that evaporization process is obtained is cooled to 30-35 degree, is then added thereto to account for its volume 3-
5% compound sedimentation agent, then crystallizes under agitation；Separation circuit is sent under conditions of stirring afterwards；The compound sedimentation agent
By ethylene glycol and glycerine according to mass ratio 5:5~7:3 mix；
（3）, separation circuit：The isolated isophthalic diformazan of twin crystal centrifuge body will be passed through by the concentrate after sedimentation operation treatment
Dimethyl phthalate -5- sulfonic acid sodium crystal, sodium sulfate crystal and mother liquor；Then by Sodium Dimethyl Isophthalate-5-sulfonate crystal
Go to refining step and carry out refinement treatment and obtain finished product, isolated mother liquor is gone into compound sedimentation agent recovery process；It is described
Twin crystal centrifuge body, including body and the Double layer rotating filter assemblies of suit are spaced in it successively, the Double layer rotating filtering
Component is co-axially mounted and is connected with motor by transmission mechanism, and filter medium wherein on internal layer rotating filter component
Aperture of the aperture more than filter medium on outer layer rotating filter component；
（4）, compound sedimentation agent recovery process：The mother liquor that separation circuit is obtained reclaims compound sedimentation agent by rectification process；Return
Compound sedimentation agent after receipts goes to step（2）Recycle.
2. Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology according to claim 1, its
It is characterised by：The mass ratio of the ethylene glycol and glycerine is 6:4.
3. Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology according to claim 1, its
It is characterised by, the step（3）In refinement treatment be to lead to isolated Sodium Dimethyl Isophthalate-5-sulfonate crystal
Cross water-washing method to be refined, the wash water in the washing comes from step（1）The steam condensate (SC) that evaporization process is obtained；It is described
Step（3）Isolated sodium sulfate crystal is refined by water-washing method, is washed the waste water for producing and is applied to step（1）'s
In Sodium Dimethyl Isophthalate-5-sulfonate technique waste water.
4. Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology according to claim 1, its
It is characterised by, the step（1）The evaporation concentration equipment that evaporization process is used is Mvr evaporators；The step（1）Middle evaporator man
It is the 35% of condensate precursor product to be evaporated Sodium Dimethyl Isophthalate-5-sulfonate technique waste water in sequence and be concentrated into volume.
5. Sodium Dimethyl Isophthalate-5-sulfonate technique waste water Comprehensive recycle technology according to claim 1, its
It is characterised by, the step（4）It is combined the bed material recovery after sedimentation agent recovery process rectification process to step（1）Isophthalic
In dicarboxylic acid dimethyl ester -5- sodium sulfonate technique waste waters.
6. according to any described Sodium Dimethyl Isophthalate-5-sulfonate technique waste water comprehensive reutilizations of claim 1-5
Technique, filter medium on the internal layer rotating filter component is screen pack, the filter medium on outer layer rotating filter component is
Filter cloth.
7. according to any described Sodium Dimethyl Isophthalate-5-sulfonate technique waste water comprehensive reutilizations of claim 1-5
Technique, it is characterised in that：The outer layer rotating filter component is 6 with the rotating ratio of internal layer rotating filter component:1.
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| CN105601031A (en) * | 2015-12-21 | 2016-05-25 | 山东省环保产业股份有限公司 | Treatment method of waste water produced during production of intermediate compound 4AA |
| CN114314996B (en) * | 2022-03-14 | 2022-06-03 | 伊沃环境科技(南京)有限公司 | Coking wastewater treatment method and device |
| CN116102469B (en) * | 2023-02-21 | 2024-04-02 | 潍坊沃尔特科技有限公司 | Waste water treatment process containing dimethyl isophthalate-5-sodium sulfonate |
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| JP4470035B2 (en) * | 2003-05-02 | 2010-06-02 | 小西化学工業株式会社 | Sulfo-substituted aromatic carboxylic acid alkyl ester and process for producing the same |
| CN1246234C (en) * | 2003-10-24 | 2006-03-22 | 南京大学 | Treatment of waste water in producing isophthalic acid dicarbomethoxy-5-sodium sulphonate and its resource utilization method |
| JP4491628B2 (en) * | 2003-11-12 | 2010-06-30 | 小西化学工業株式会社 | Method for producing alkali salt of sulfo-substituted aromatic carboxylic acid alkyl ester |
| CN103881006B (en) * | 2014-04-01 | 2016-06-29 | 山东宝莫生物化工股份有限公司 | Large arch dam high molecular weight anionic modified polyacrylamide reversed emulsion polymerization |
| CN104003910B (en) * | 2014-06-13 | 2016-06-29 | 山东金盛新材料科技有限公司 | The method extracting 5-sodium sulfo isophthalate waste water is produced from three monomers |
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